Azatadine synthesis
- Product Name:Azatadine
- CAS Number:3964-81-6
- Molecular formula:C20H22N2
- Molecular Weight:290.4
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Yield: 87.5%
Reaction Conditions:
with palladium 10% on activated carbon;hydrogen;acetic acid in ethanol at 60; for 20 h;Solvent;Temperature;Reagent/catalyst;
Steps:
1-4 The loratadine impurity (Formula II) is prepared using the following steps:
To a 100mL three-necked flask, add methylloratadine (3.25g, 10mmol, 1.0eq) and ethanol (25mL), then add acetic acid (1.2g, 20mmol, 2.0eq) and 10% palladium on carbon (1.60g, 1.5mmol) , 0.15eq). Then evacuate, replace with hydrogen three times, and finally raise the temperature to 60 ° C in a hydrogen balloon atmosphere, stir the reaction for 20 hours, drop to room temperature, filter to remove the palladium carbon, concentrate, and the residue is purified by silica gel column chromatography to obtain loratadine impurities 2.54g, yield 87.5%, HPLC purity 99.57%.
References:
Shenzhen Xianggen Biological Technology Co., Ltd.;He Dongmei;Li Fanglin;Zhuang Shibin;Peng Jinan CN110845475, 2020, A Location in patent:Paragraph 0029-0052
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